[2-(4-Acetylamino-phenyl)-1,3-dihydroxy-indan-2-yl]-acetic acid ethyl ester → [2-(4-Acetylamino-phenyl)-indan-2-yl]-acetic Acid Ethyl Ester

HRID 1375080노트

반응식

HRID 1375080 반응식
[CH2:1]([O:3][C:4](=[O:27])[CH2:5][C:6]1([C:17]2[CH:22]=[CH:21][C:20]([NH:23][C:24](=[O:26])[CH3:25])=[CH:19][CH:18]=2)[CH:14](O)[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH:7]1O)[CH3:2]>C(O)(=O)C.[Pd]>[CH2:1]([O:3][C:4](=[O:27])[CH2:5][C:6]1([C:17]2[CH:18]=[CH:19][C:20]([NH:23][C:24](=[O:26])[CH3:25])=[CH:21][CH:22]=2)[CH2:7][C:8]2[C:13](=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH2:14]1)[CH3:2]

참가 물질

4

반응물 1

HCID 69417565[2-(4-Acetylamino-phenyl)-1,3-dihydroxy-indan-2-yl]-acetic acid ethyl ester

생성물 1

HCID 69418529[2-(4-Acetylamino-phenyl)-indan-2-yl]-acetic Acid Ethyl Ester수율 85.3%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

반응 조건

온도
50 °C

실험 절차

A stirred solution of [2-(4-acetylamino-phenyl)-1,3-dihydroxy-indan-2-yl]-acetic acid ethyl ester (0.38 g, Reference Example 12) in acetic acid (20 mL), under nitrogen, was treated with palladium black (20 mg), then the flask was evacuated and then hydrogen was introduced into the flask via a balloon. After stirring at 50° C. for 2 days the reaction mixture was filtered through Hi-flow supercel. The filtrate was concentrated then diluted with ethyl acetate (100 mL). This solution was washed with saturated sodium hydrogen carbonate solution (100 mL), then with water (100 mL), then dried over magnesium sulfate and then evaporated to give the title compound (0.296 g) as an amber coloured gum.

후처리

  1. customthe flask was evacuated
  2. additionhydrogen was introduced into the flask via a balloon
  3. filtrationwas filtered through Hi-flow supercel
  4. concentrationThe filtrate was concentrated
  5. additionthen diluted with ethyl acetate (100 mL)
  6. washThis solution was washed with saturated sodium hydrogen carbonate solution (100 mL)
  7. dry with materialwith water (100 mL), then dried over magnesium sulfate
  8. customevaporated

출처 및 근거

ORD 기록
ord-5cf2621d0b174eabad1f770dd5f890fd
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07166616B2

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